Matrix solid phase dispersion isolation and liquid chromatographic determination of oxytetracycline in catfish (Ictalurus punctatus) muscle tissue.
A method for isolation and liquid chromatographic determination of oxytetracycline in catfish (Ictalurus punctatus) muscle tissue is presented. Blank control and oxytetracycline-fortified fish muscle tissue samples (0.5 g) were blended with octadecylsllyl (C18, 40 microns, 18% load, endcapped) derivatized silica packing material (2 g) containing 0.05 g each of oxalic acid and disodium ethylenediaminetetraacetate. A column made from the C18/fish tissue matrix was first washed with hexane (8 mL), following which the oxytetracycline was eluted with acetonitrile-methanol (1 + 1, v/v) containing 0.06% w/v each of butylated hydroxyanisole and butylated hydroxytoluene. The eluate contained oxytetracycline analyte that was free from interfering compounds when analyzed by liquid chromatography with UV detection (photodiode array set at 365 nm). Standard curves for oxytetracycline isolated from fortified samples were linear (0.998 +/- 0.002) with an average absolute percentage recovery of 80.9 +/- 6.6% for the concentration range (50, 100, 200, 400, 800, 1600, and 3200 ng/g) examined. The interassay variability was 11.3 +/- 5.2% with an intra-assay variability of 1.1%.
Long
A R
AR
Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology, and Toxicology, Baton Rouge 70803.
Hsieh
L C
LC
Malbrough
M S
MS
Short
C R
CR
Barker
S A
SA
D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D007059:Ictaluridae / Q000378:metabolism*; D009132:Muscles / Q000737:chemistry; D010118:Oxytetracycline / Q000032:analysis* / Q000302:isolation & purification
D010118:Oxytetracycline